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4'-Hydroxy-4-biphenylcarbonitrile → 4-(3-Hydroxy-propoxy)-benzoic acid 4'-cyanobiphenyl-4-yl ester

HRID 890901
Notes
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Reaction equation

HRID 890901 reaction equation
[Si]([O:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:21]=[CH:20][C:16]([C:17]([OH:19])=[O:18])=[CH:15][CH:14]=1)(C(C)(C)C)(C)C.O[C:23]1[CH:28]=[CH:27][C:26]([C:29]2[CH:34]=[CH:33][C:32]([C:35]#[N:36])=[CH:31][CH:30]=2)=[CH:25][CH:24]=1>C(Cl)Cl>[C:35]([C:32]1[CH:33]=[CH:34][C:29]([C:26]2[CH:25]=[CH:24][C:23]([O:19][C:17](=[O:18])[C:16]3[CH:15]=[CH:14][C:13]([O:12][CH2:11][CH2:10][CH2:9][OH:8])=[CH:21][CH:20]=3)=[CH:28][CH:27]=2)=[CH:30][CH:31]=1)#[N:36]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 1406104'-Hydroxy-4-biphenylcarbonitrileHCID 222424964-(3-{[tert-Butyl(dimethyl)silyl]oxy}propoxy)benzoic acid

Product 1

HCID 235977644-(3-Hydroxy-propoxy)-benzoic acid 4'-cyanobiphenyl-4-yl esterYield 89%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
40 °C

Procedure

To a solution of 2 (10 g, 32.21 mmol), 4′-hydroxy-biphenyl-4-carbonitrile (6.35 g, 32.53 mmol), and toluenesulfonic/4-(dimethylamino)pyridine complex (0.95 g, 3.22 mmol) in anhydrous methylene chloride (100 mL) was added N,N-dicyclohexylcarbodiimide (6.98 g, 33.82 mmol) under argon. The reaction mixture was stirred at 40° C. overnight. Upon filtering off the white residues, the filtrate was diluted with additional methylene chloride. The solution was then washed with water. The silyl ether of the title compound was purified by flash column chromatography on silica gel with gradient elution from 0 to 2% acetone in methylene chloride. The silyl-protected compound was hydrolyzed in tetrahydrofuran: water:acetic acid (80 mL: 80 mL: 240 mL) overnight. The volume of the solution was reduced by 50% via evaporation under reduced pressure. Methylene chloride was added to the slurry for washing sequentially with H2O, a 10% NaHCO3 solution and brine before drying over anhydrous MgSO4. The crude product resulting from evaporation of the solvent was purified by recrystallization from ethanol to yield 3 (10.71 g, 89%). 1H NMR spectral data (400 MHz, CDCl3): δ 2.10 (quintet, 2H, —CH2—), δ 3.95 (t, 2H, —CH2OAr), δ 4.25 (t, 2H, HOCH2—), δ 7.00–8.25 (m, 12H, aromatic rings).

Workup

  1. filtrationUpon filtering off the white residues
  2. additionthe filtrate was diluted with additional methylene chloride
  3. washThe solution was then washed with water
  4. customThe silyl ether of the title compound was purified by flash column chromatography on silica gel with gradient elution from 0 to 2% acetone in methylene chloride
  5. customacetic acid (80 mL: 80 mL: 240 mL) overnight
  6. customThe volume of the solution was reduced by 50% via evaporation under reduced pressure
  7. additionMethylene chloride was added to the slurry
  8. washfor washing sequentially with H2O
  9. dry with materiala 10% NaHCO3 solution and brine before drying over anhydrous MgSO4
  10. customThe crude product resulting from evaporation of the solvent
  11. customwas purified by recrystallization from ethanol

Sources & evidence

ORD record
ord-b13dda1bfc7e4c2aa09ea5f393f5a97a
Source dataset
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07001648B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes